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By

Srinivasulu P 08ETMM02

Title of the M. Tech Dissertation

School of Engineering Sciences & Technology (SEST) University of Hyderabad

Estimation of -transus temperature in an alloy based on Ti-6Al-4V

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Supervisor Dr. Koteswararao V. Rajulapati

School of Engineering Sciences & Technology, UOH.

Introduction

I think it is best to choose such a denomination as means nothing of itself and thus can give no rise to any erroneous ideas. In consequence of this, as I did in the case of Uranium, I shall borrow the name for this metallic substance from mythology, and in particular from the Titans, the first sons of the earth. I therefore call this metallic genus TITANIUM. - Martin Heinrich Klaproth (1795) Titanium and titanium alloys three major categories (according to the predominant phases present in their microstructure) : , + and alloys. The transformation temperature from + or from to all is known as the -transus temperature (tr). Pure titanium undergoes an allotropic transformation (-HCP to -BCC) at 8822 oC. S E S T

The transus is an important parameter to be considered during the design of


thermo-mechanical processing schedules since a variety of microstructures can be obtained depending upon whether the material is processed above or below this temperature.
Continued
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Objectives of the present investigation


To estimate transus temperature, by performing heat treatment procedures for Ti-6Al4V and Ti-6Al-1.5V-2.5Cu alloys at 900 oC, 950 oC, 1000 oC respectively. Performing metallographic procedures to obtain microstructures in order to estimate the transus temperature. The microstructures are analyzed by stereographic techniques to quantify the transformed phases for different sample conditions at different temperatures (Image analysis-Optical microscopy). Study on X-ray diffraction results of alloy samples and correlate them with existing phases during heat treatments. Remarks on the obtained measurements of micro-hardness.

Introduction
(continued..)

Objectives of the Project

Literature Review

Titanium alloys and their classification Crystal structures of titanium alloys Phase transformations in titanium alloys Principles of alloying and alloying titanium Effect of alloying additions on -transus temperature in titanium alloys Effect of alloying Al, V additions on -transus in Ti-6Al-4V alloy Overview of high pure Ti, Ti-6Al-4V and Ti-6Al-1.5V-2.5Cu alloys S E S T

(a)

Widmansttten
continued
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Literature Review
(continued)
Titanium with oxygen, AluminumIncrease in transus temperature (Interstitial & substitutional effects) Titanium with vanadium, Copper- decrease in transus temperature (substitutional solid solution strengthening , precipitation hardening) Titanium with Zirconium and Tin- there is no change in transus temperature (Neutral)
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Effect of Al, V alloying additions on transus temperature in Ti-6Al-4V alloy: * Due to the addition of Vanadium (V) content at constant Aluminum (Al) concentration, there is a rapid decrease in the (+)/ transformation temperature (i.e. transus) and it does not significantly influence the position of / (+) transformation temperature (i.e. transus).

Heat treatments for titanium alloys

Variation of transus temperature with stabilizers

Literature Review
(continued)
Heat treatments for titanium alloys Titanium alloys- effects of stabilizing elements on transus and phase stabilization stabilizing effect of Mo/V/Nb/Ta --> 10/6.7/2.8/2.2 (wt%) ----------------------------------------------------------------- Stabilizer Approx. wt% needed to retain 100% upon quenching ------------------------------------------------------------------------------------Mo Isomorphous 10 V Isomorphous 15 W Isomorphous 22.5 Nb Isomorphous 36.0 Ta Isomorphous 45.0 Fe Eutectoid 3.5 Cr Eutectoid 6.5 Cu Eutectoid 13.0 Ni Eutectoid 9.0 ------------------------------------------------------------------------------------Type

S E S T

continued

The stability of a phase is determined by binding energy at absolute zero and the entropy of the system. During heat treatment, the free energy of an imaginary bcc lattice will decrease

more rapidly than those of the competing alternatives such that eventually a temperature will be reached where at the lattice will transform from the low

temperature stable closed packed structure to bcc.


Stability of a phase: HCP () and BCC () structures For the relatively loose bcc packing and atoms within the lattice easier to move,

this may result in high amplitude of vibration in certain directions, and the resulting contribution to -TS term of the free energy. At high temperatures, F= H-TS is small. Upon cooling from the phase field the most densely packed planes of the bcc

phase {110} transform to the basal planes {0001} of the hexagonal phase. Titanium HCP phase is stable at lower temperatures, because it has the higher

binding energy, where entropy effects are unimportant.


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continued

Experimental work

Metallographic preparations Heat treatments Materials: Ti-6Al-4V Ti-6Al-1.5V-2.5Cu Image analysis- Optical X-ray diffraction analysis Vickers Micro hardness Naskar muffle furnace
(27 1400 oC)

S E S T

Optical microscopy

Heat treated specimen Bruker D8 XRD system

Details of operation- Optical microscope: for quantitative phase analysis

Operating parameters for X-ray diffraction:


Incident radiation: Cu k1, = 1.5418 Ao Sample type: Flat bulk thin in polished and etched Sample Dimensions: Plate or bar shape and 15 mm-7 mm-4 mm Scan mode: Step mode Step size: 0.1-0.2 o (depend on dimensions of the sample) Scan speed: 1 step/sec Scan angle (vertical theta) range: 20-120 o

Experimental details
(continued..)
Metallurgical specimen preparation:

Mirror-like finish of the specimen is needed Remove oxide layer with rough polishing
for X-ray diffraction:

Apparatus model: Olympus GX 51 compact inverted metallurgical microscope Mode of illumination: Halogen (optical transmitted) illumination Mode of examination: Bright field and simple polarization mode Magnification range: 50X-1000X

Heat treatments performed in the present work:

Flat & thin samples could be used

Calibration of XRD Instrument is must before doing experiment

As-cast Ti-6Al-4V HT at 900, 950 and 1000 oC and then furnace cooled, water-quenched. Soak time 2 hours and cooling rate 15 oC/sec. As-cast Ti-6Al-1.5V-2.5Cu HT at 900, 950 and 1000 oC and then furnace cooled, water-quenched. Soak time 2 hours and cooling rate 15 oC/sec.

Operating temp. range: RT 1400 oC Model name: Electro heat-Naskar muffle furnace Temp. measurements: Thermo couple Thyrister current range: 14-25 amps Operating atmosphere: Open, Not any inert gas atmosphere Etchant: 50 ml diluted solution-Krolls reagent (2 ml HF-40% Con., 3 ml HNO3-60-65% con., 1.5 ml H2O2 and 45 ml H2O) 9

Heating muffle furnace operation:

Process flow-chart for Image analysis:

Experiment work (continued)

Continued

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Results and Discussion


Phase disappearing method Microstructural analysis-

Optical microscopy Quantitative phase analysis- XRD Remarks on Vickers microhardness

Phase disappearing method: A series of two phase (+) alloys are equilibrated at a given temperature or solutionized, quenched to room temperature. By thermal arrest technique the retained phase measured through the help of microstructures and as well as XRD. According to Lever rule at the / (+) solvus line, the amount of is zero. This solvus temperature determines the transus temperature and it is 890 oC for commercially pure titanium, and for Ti-6Al-4V and Ti-6Al-1.5V-2.5Cu alloys it lies between 970 oC to 1005 oC, from the sequential investigations done by S Gollapudi et.al.

S E S T

Microstructures of as-cast Ti-6Al-4V alloy ( Coarse, heterogeneous Microstructure; dark phase- and bright phase- ) continued

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Lath-like Widmansttten morphology consists of plates At intermediate cooling rates or furnace cooling from phase field the resultant Widmansttten structures are produced.

Microstructures of Ti-6Al-4V Heat treated at 900 oC then furnace cooled

S E S T

Fine acicular martensite structure.


Partial disordered array of individual platelets and phase is parallel to {110} planes of matrix.

Microstructure of Ti-6Al-4V alloy heat treated at 900 oC, and then water- quenched continued
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Theoretically predicted Widmansttten morphology with recrystalized platelets surrounded by prior boundaries. Basket-weave within Widmansttten structure. The basket-weave structure results from nucleation and growth during the transformation of to in a Widmansttten pattern The distribution of smaller and finer colonies is due to the characteristic nature of basketweave structures S E S T

Microstructures of Ti-6Al-4V Heat treated at 950 oC then furnace cooled

Microstructure of Ti-6Al-4V alloy heat treated at 950 oC, and then water- quenched continued
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The microstructure exhibits the fine lamellae delineating by phase boundary.

Microstructures of Ti-6Al-4V Heat treated at 1000 oC then furnace cooled The microstructure is needle like lamellar HCP martensite

S E S T

At higher cooling rates, Ti6Al-4V can form Hexagonal closed packed martensite () which contains vanadium supersaturaion.
Microstructure of Ti-6Al-4V alloy heat treated at 1000 oC, and then water- quenched continued
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For Ti-6Al-4V alloy, the maximum retained phase fractions are measured and observed at 1000 oC then water-quenched, and it is 81.17%

For Ti-6Al-1.5V-2.5Cu alloy, the maximum retained phase fractions are measured and observed at 950 oC then waterquenched, and it is 75.35%

S E S T

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The commercial Ti-6Al-1.5V-2.5Cu alloy is also an + eutectoid titanium alloy. Copper is one such -eutectoid stabilizing element and intermetallic compound former in titanium alloys Just like silicon, Cu can also be added to titanium, by forming a Ti-Cu system that An intermetallic precipitation (Ti2Cu) in the vicinity of dislocations acts to obstruct their movement, improving the systems creep resistance. exhibits precipitation-strengthening. As the temperature decreases, the solid solubility of this system too decreases, precipitating Ti2Cu. S E S T

Microstructures of as-cast Ti-6Al-1.5V-2.5Cu alloy

continued

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copper precipitates appeared in the form of newly grown crystalline morphology i.e. serrated or elongated lamellae Basket-weave Widmansttten structure and the lamellar structure is indeed present among the lamellae A mixture of and Cu diluted phase representing the uniformed surface without any phases into the matrix of phase. There is also a secondary observed in the micrographs Microstructure of Ti-6Al-1.5V-2.5Cu alloy heat treated at 900 oC, and then waterquenched continued
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Microstructures of Ti-6Al-1.5V-2.5Cu Heat treated at 900

oC

then furnace cooled

S E S T

In these microstructures the transformation product is most commonly recognized in the form of colonies of what appeared to be alternating and almost parallel strips of two-phase products

Microstructures of Ti-6Al-1.5V-2.5Cu Heat treated at 950


Martensitic transformed phase as in the form of needle like phase or fine acicular phase. The intergranular morphology also martensitic phase product in the form of fine or acicular structure. This is good for wear resistance

oC

then furnace cooled

S E S T

Microstructure of Ti-6Al-1.5V-2.5Cu alloy heat treated at 950 oC, and then waterquenched continued
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Homogeneous microstructure is produced by furnace cooling from 1000 oC. There is a fine grain boundary separating the and and internal structures. It reveals that there is no secondary phase product form

Microstructures of Ti-6Al-1.5V-2.5Cu Heat treated at 1000

oC

then furnace cooled

S E S T

The structure is fully populated with the Widmansttten arrangement of platelets

Microstructure of Ti-6Al-1.5V-2.5Cu alloy heat treated at 1000 oC, and then waterquenched continued
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XRD profiles of Ti-6Al-4V alloy Ti-6Al-4V HT 1000 o C then waterquenched alloy XRD Braggs pattern contain no reflections.

S E S T

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S E XRD profiles of Ti-6Al-1.5V-2.5Cu S alloy T

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Vickers Micro hardness

The maximum Vickers hardness value (in no.) of Ti-6Al-4V attain at 900 oC, furnace cooled condition ( Surface effects more during slow cooling) The maximum Vickers hardness value (in no.) of Ti-6Al-1.5V-2.5Cu attain at 1000 oC, water-quenched condition (Precipitation hardening effect)

S E S T

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Conclusion
Processing Metallographic Evaluation: Phase analysis Estimation of transus

The objective was to estimate the transus temperature by traditional metallographic techniques or procedures i.e. phase disappearing method via microscopic methods as well as X-ray diffraction phase analysis. Through the subtransus or transus processing, varying microstructural features such as morphology and phase transformations can be reviewed in Ti-6Al-4V and Ti6Al-1.5V-2.5Cu alloys. Ti-6Al-4v alloy specimens are heat treated at 900, 950 and 1000 oC and then furnace cooled, the measurements of retained phase fractions, obtained from microstructural analysis, are as 65.72%, 59.08 % and 69.28% respectively. Ti-6Al-4V alloy specimens are heat treated at 900, 950 and 1000 oC and then S E S T

temperature for Ti-6Al-4V and


Ti-6Al-1.5V-2.5Cu alloys Mechanical behavior: Vickers hardness of Ti-6Al-4V and Ti-6Al-1.5V-2.5Cu alloys

water-quenched, the measurements of retained phase fractions, obtained from

microstructural analysis, are 64.68%, 62.20% and 81.17% respectively.


Continued
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Ti-6Al-1.5V-2.5Cu alloy specimens are heat treated at 900, 950 and 1000 oC and

then furnace cooled, from quantification of phase by microstructural analysis, the retained phase is found to be 60.65%, 63.31% and 67.47% respectively. Ti-6Al-1.5V-2.5Cu alloy specimens are heat treated at 900, 950 and 1000 oC and

then water-quenched, from quantification of phase by microstructural analysis, the


retained phase is found to be 60.95%, 75.35% and 55.53% respectively.

The estimated transus temperature in Ti-6Al-4V alloy is 1000 15 oC and it is greater than the transformation temperature of Pure titanium i.e., 882 2 oC

The estimated transus temperature in Ti-6Al-4V alloy is 950 25 oC and it is


greater than the transformation temperature of Pure titanium i.e., 882 2 oC
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Continued to acknowledgements

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Acknowledgements
Thanks to..
Dr. Koteswararao V. Rajulapati Prof. Sundararaman Mahadevan, Dean, SEST Prof. Rajendra Singh, School of Physics Dr. Dibakar Das, SEST

Prof. V Krishna, School of Humanities


............................................. Prof. Anil. K. Bhatnagar, UOH

Dr. V.S Raghunathan


Dr. Vadali. V. S. S. Srikanth, SEST
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